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Article history: ZnO nanoparticles (ZnO-NPs) were prepared by a solegel combustion method from a zinc acetate
Received 19 April 2010 precursor and acetic acid. The ZnO-NPs were synthesized at calcination temperatures of 650 C and
Received in revised form 750 C for 1 h. The synthesized ZnO-NPs were characterized by X-ray diffraction analysis (XRD) and TEM.
6 November 2010
The XRD results revealed that the sample product was crystalline with a hexagonal wurtzite phase. High-
Accepted 17 November 2010
Available online 24 November 2010
magnification transmission electron microscopy (TEM) showed single-crystal ZnO-NPs with nearly
spherical shapes. The crystalline development in the ZnO-NPs was investigated by X-ray peak broad-
ening. The WilliamsoneHall (WeH) analysis and sizeestrain plot method were used to study the indi-
Keywords:
X-ray analysis
vidual contributions of crystallite sizes and lattice strain on the peak broadening of the ZnO-NPs. The
ZnO physical parameters such as strain, stress and energy density values were calculated more precisely for
Nanoparticle all the reflection peaks of XRD corresponding to the wurtzite hexagonal phase of ZnO lying in the range
Solegel synthesis of 20 e100 from the modified form of the WeH plot assuming a uniform deformation model (UDM),
uniform stress deformation model (USDM), uniform deformation energy density model (UDEDM) and by
the sizeestrain plot method (SSP). The results obtained showed that the mean particle size of the ZnO-
NPs estimated from the TEM, WeH analysis and the SSP method were highly intercorrelated.
Ó 2010 Elsevier Masson SAS. All rights reserved.
1293-2558/$ e see front matter Ó 2010 Elsevier Masson SAS. All rights reserved.
doi:10.1016/j.solidstatesciences.2010.11.024
252 A. Khorsand Zak et al. / Solid State Sciences 13 (2011) 251e256
2. Experimental
Table 1
The structure parameters of ZnO-NPs calcinated at 650 C and 750 C.
Plots were drawn with 1/bD on the x-axis and cosq along the
y-axis for the ZnO-NPs prepared at different temperatures such
that the preferred orientation peaks of ZnO with the wurtzite
hexagonal phase appeared between 2q ¼ 20 and 100 . By fitting
the data, the crystallite size D was extracted from the slope of the
fit line; see Fig. 3.
kl
bhkl ¼ þ ð43tanqÞ (7)
Dcosq
Rearranging Eq. (7) gives:
kl Fig. 4. The WeH analysis of ZnO-NPs calcinated at 650 C and 750 C assuming UDM.
bhkl cosq ¼ þ ð43sinqÞ (8) Fit to the data, the strain is extracted from the slope and the crystalline size is extracted
D
from the y-intercept of the fit.
254 A. Khorsand Zak et al. / Solid State Sciences 13 (2011) 251e256
Fig. 5. The modified form of WeH analysis assuming USDM for ZnO-NPs calcinated at
650 C and 750 C. Fit to the data, the stress is extracted from the slope and the
crystalline size is extracted from the y-intercept of the fit. Fig. 6. The modified form of WeH analysis assuming UDEDM for ZnO-NPs calcinated
at 650 C and 750 C. Fit to the data, the density of energy is extracted from the slope
Eq. (8) represents the UDM, where the strain was assumed to be and the crystalline size is extracted from the y-intercept of the fit.
kl 4ssinq
bhkl cosq ¼ þ (9)
D Yhkl
estimated from the slope of these lines, and the crystallite size D
from the y-intercept; see Fig. 6. Previously, we had s ¼ 3Y and
u ¼ (32Yhkl)/2, where the stress s was calculated as u ¼ (s2/2Yhkl).
The results of these plots show a slight change in energy density
of the ZnO-NPs with increasing calcination temperature.
2 K 2 3 2
ðdhkl bhkl cosqÞ ¼ dhkl bhkl cosq þ (12)
D 2
Table 2
Geometric parameters of ZnO-NPs calcinated at 650 C and 750 C.
D D 3 no D (nm) 3 no s D 3 no s u D 3 no s u D
(nm) (nm) unit 103 unit 103 (MPa) (nm) unit 103 (MPa) (KJm3) (nm) unit 103 (MPa) (KJm3) (nm)
650 18.58 16.19 1.2006 16.57 0.9867 125.31 16.34 1.1015 139.90 77.051 15.97 1.1843 150.41 89.681 e
750 22.54 18.55 0.9302 18.77 0.8611 109.36 18.91 0.8104 102.92 41.702 17.69 0.8908 113.13 50.393 ∼20
256 A. Khorsand Zak et al. / Solid State Sciences 13 (2011) 251e256
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characterized by powder XRD and TEM. The XRD indicated that 591.
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